5H-［1，2，3］三唑并［4，5-c］呋咱及其含能衍生物的合成

摘要

A novel nitrogen-rich energetic material 5H-[1,2,3]triazolo[4,5-c][1,2,5]oxdiazole(2) was prepared via hydrolytic reac-tion using [1,2,5]oxadiazole [3,4-e][1,2,3,4]tetrazine 4,6-di-N-oxide(FTDO) as raw material.Four new energetic derivatives, am-monium [1,2,3]triazolo [4,5-c][1,2,5]oxdiazole(3), hydrazinium [1,2,3]triazolo[4,5-c][1,2,5]oxdiazole(4), guanylureaium [1,2,3]triazolo[4,5-c][1,2,5]oxdiazole(5) and triaminoguanidinium [1,2,3] triazolo[4,5-c][1,2,5]oxdiazole(6) were designed and synthesized via reactions of compound 2 with ammonia gas, hydrazine hydrate, amidinothiourea hydrochloride and triaminogunidine nitrate, respectively.Their structures were characterized by IR, NMR and elemental analysis.The mechanism and conditions of hydrolytic reaction were analyzed.The optimal reaction conditions were determined as:the reaction time 5 h and reaction tempera-ture 80 ℃with a yield of 76.92%.The thermal properties of compounds, 2,4,5 and 6, were analyzed by DSC.Results show that their peak temperatures of initial decomposition reaction are 173.23, 144.82, 172.81, 164.94 ℃, respectively.%以呋咱并[3，4-e]-1，2，3，4-四嗪-4，6-二氧化物（FTDO）为原料，经水解反应合成了新型富氮含能材料5H-[1，2，3]三唑并[4，5-c]呋咱（2），然后与氨气、水合肼、脒基脲盐酸盐、三氨基胍硝酸盐反应合成了[1，2，3]三唑并[4，5-c]呋咱铵盐（3）、[1，2，3]三唑并[4，5-c]呋咱肼盐（4）、[1，2，3]三唑并[4，5-c]呋咱脒基脲盐（5）和[1，2，3]三唑并[4，5-c]呋咱三氨基胍盐（6）4种新的含能衍生物，并采用红外光谱、核磁共振光谱、元素分析等进行了结构表征；探讨了水解反应的机理和条件，确定最佳条件为：80℃下反应5 h，收率为76．92％；采用DSC热分析手段研究了化合物2、4、5和6的热性能，其初始分解峰温分别为173．23，144．82，172．81，164．94℃。